US9221047B2 - Device for controlled distribution of micro- or nano-volumes of a liquid based on the piezoelectric effect in functionalized materials, without using external electric sources - Google Patents

Device for controlled distribution of micro- or nano-volumes of a liquid based on the piezoelectric effect in functionalized materials, without using external electric sources Download PDF

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US9221047B2
US9221047B2 US13/265,720 US201013265720A US9221047B2 US 9221047 B2 US9221047 B2 US 9221047B2 US 201013265720 A US201013265720 A US 201013265720A US 9221047 B2 US9221047 B2 US 9221047B2
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substrate
liquid
starting
pyroelectric
top surface
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US20120112070A1 (en
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Pietro Ferraro
Sara Coppola
Veronica Vespini
Simonetta Grilli
Melania Paturzo
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Consiglio Nazionale delle Richerche CNR
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/02Burettes; Pipettes
    • B01L3/0241Drop counters; Drop formers
    • B01L3/0262Drop counters; Drop formers using touch-off at substrate or container
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/02Burettes; Pipettes
    • B01L3/0241Drop counters; Drop formers
    • B01L3/0268Drop counters; Drop formers using pulse dispensing or spraying, eg. inkjet type, piezo actuated ejection of droplets from capillaries
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41JTYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
    • B41J2/00Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
    • B41J2/005Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277Apparatus
    • B01J2219/00351Means for dispensing and evacuation of reagents
    • B01J2219/00378Piezoelectric or ink jet dispensers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00Additional constructional details
    • B01L2300/08Geometry, shape and general structure
    • B01L2300/0809Geometry, shape and general structure rectangular shaped
    • B01L2300/0819Microarrays; Biochips
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00Moving or stopping fluids
    • B01L2400/04Moving fluids with specific forces or mechanical means
    • B01L2400/0403Moving fluids with specific forces or mechanical means specific forces
    • B01L2400/0415Moving fluids with specific forces or mechanical means specific forces electrical forces, e.g. electrokinetic
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00Moving or stopping fluids
    • B01L2400/04Moving fluids with specific forces or mechanical means
    • B01L2400/0403Moving fluids with specific forces or mechanical means specific forces
    • B01L2400/0442Moving fluids with specific forces or mechanical means specific forces thermal energy, e.g. vaporisation, bubble jet
    • B01L2400/0448Marangoni flow; Thermocapillary effect

Definitions

  • the present invention concerns an electro-dynamical dispenser of liquids in micro-/nano volumes based on the pyroelectric effect in functionalized materials without using an external electrical field.
  • the present invention concerns the production and the distribution of pico and nano-drops which are extracted, by the effect of a strong electric field generated by pyroelectric effect, in particular, but not exclusively, by a sessile drop (a drop placed on a surface assumes a form named “sessile”) or by a liquid film, and distributed on a dielectric substrate.
  • the electric field is advantageously generated by applying a heat source on the substrate of interest or utilizing a laser source emitting at infrared region.
  • a variety of functions, useful in micro-fluid and opto-fluid systems such as the adaptation of the liquid meniscus form, the spatial geometric modulation or “patterning”, the shifting and drop formation [1-5-19], may be performed by different approaches, for example the “electro-wetting” (EW) or the thermo-capillary [2-20-21].
  • EW electro-wetting
  • thermo-capillary thermo-capillary
  • microfluidic systems are essentially based on hydrodynamic forces whereas the approaches assisted by electric field became more and more popular only recently, due to their advanced flexibility and their additional functionality [22-23].
  • the formation of micro- or nano-liter drops caused by electric field is useful in electro-spray mass spectroscopy, injkjet printing, biomolecular manipulation [16] that furnishes a so-called “on demand” distribution of material [7-15].
  • EHD electro-dynamic approach
  • the EHD method requires the application of high voltages (e.g. in the “e-jet printing”), usually between the nozzle and the distribution plate, so as to allow the flow of fluid and its distribution on the substrate under examination.
  • photo-lithographic methods are not easily used for such materials and, in the current situation, methods are not available that are characterized by high flexibility, simplicity and low cost, so as to permit easy change in the type of structure to be realized.
  • the first of the three previous mentioned works demonstrates the creation of a group of little drops spatially arranged on a surface starting from a liquid film. These drops function as a lens.
  • the second work demonstrates the use of such drops for non-optical purposes, for example for chemical and biological experimentation at nano-metric levels.
  • the third work demonstrates the mentioned creation of drops starting, this time, from a liquid polymer by means of a thermal stimulus.
  • This thermal stimulus simultaneously provides for the “linking” of the same polymer, impressing a regular geometric configuration (“pattern”) to the polymer, and thus a lithographic method is obtained, in such a way.
  • It is the object of the present invention is to provide a method for the distribution of pico- or nanodrops of a material on a dielectric substrate, that solves the problems and overcomes the drawbacks of the prior art.
  • An additional specific object of the present invention is an apparatus that uses the method object of the invention.
  • An additional specific object of the present invention is the use of the apparatus, object of the invention, for printing.
  • the subject-matter of the present invention is a method for the controlled distribution of pico- or nano-volumes of a liquid, comprising the step of:
  • the pyroelectric surface has been obtained modifying its wettability.
  • the mentioned pyroelectric substrate is Lithium Niobate z-cut or Lithium Tantalate.
  • the heating is performed selectively on the surface of the pyroelectric substrate.
  • the heating is effected by infrared Laser or any source of electromagnetic radiation.
  • the heating is effected by means of a movable heated tip.
  • the pyroelectric substrate has been functionalized by creating periodic polarized structures, in correspondence of which one has deposed sessile drops, to obtain a surface charge distribution with charge having alternated sign and pre-defined geometry.
  • the movable heat source is moved in such a way that, when the off-the-axis distribution angles of the liquid are larger than a threshold value ⁇ that is function of the liquid type, of the material on which the sessile drop is put down and of the type of electric charge distribution on the pyroelectric substrate, the sessile drop moves, whilst when the off-the-axis distribution angle is smaller than said threshold value, the sessile drop keep fixed and the liquid can be distributed within this cone having apex angle ⁇ .
  • a threshold value ⁇ that is function of the liquid type, of the material on which the sessile drop is put down and of the type of electric charge distribution on the pyroelectric substrate
  • the laser beam is separated in such a way that a plurality of spatially separated beams incise simultaneously on the pyroelectric substrate, thus creating a simultaneous emission of liquid from multiple sessile drops or different points of the liquid film.
  • the wettability is with poling processes and thermal stimuli.
  • the pyroelectric substrate is the destination substrate.
  • the liquid to be distributed is any liquid which reacts to an applied electrical field, in particular chosen in the group consisting of: almond oil, poly-dimethyl-siloxane (PDMS).
  • PDMS poly-dimethyl-siloxane
  • a PDMS liquid layer is put down on the starting substrate, creating, on the destination substrate, through its selective heating hanging drops in correspondence of the surface hexagons of the same pyroelectric substrate.
  • the starting substrate is glass.
  • the starting substrate is the pyroelectric substrate.
  • the starting and destination substrates are pyroelectric, being both heated, therefore, they receive the liquid from the surface of the opposite substrate.
  • Further specific subject-matter of the present invention is a method for the controlled distribution of pico- or nano-volumes of a liquid, comprising the step of:
  • Additional specific object of the present invention is a device for the controlled distribution of pico- or nano-volumes of a liquid, comprising:
  • the device comprises a third substrate, that is dielectric, the second substrate being interposed in a movable way parallel to said third substrate, so as to intercept the liquid being distributed, in such a case the surface of the destination substrate is set at a distance D calculated between the surface of the starting substrate and the surface of the interposed substrate.
  • the starting substrate includes through micro-holes and micro-tubes for dosing the distribution liquid in the sessile drops.
  • the liquid is sucked by suction channels if an immediate interruption of the distribution is wished.
  • the destination substrate surface is set at a distance D from the starting substrate surface by means of electrically insulating spacers.
  • FIG. 1 shows in (a) and (b) a diagram of the apparatus according to the invention, in two different embodiments of invention; in (c) a bi-dimensional plot of the electric field lines (left) and of electric potential (right) obtained with by a finite-elements simulation method of finished elements; in (d) a typical liquid bridge and in (e)-(f) typical discharges of the liquid, respectively, with almond oil and PDMS;
  • FIG. 2 shows: in (a) a sequence of different discharges of distribution in case of liquid film and thermal stimulus inducted through by the heated tip; in (b) a sequence of different discharges of distribution in case of sessile drops and thermal stimulus inducted through by infrared laser; in (c) a plot of the volume transfer percentage concerning the FIG. 2( a ) (square box) and a plot of the height variation during the time (principal plot); in (d) a plot of the volume transfer percentage concerning the FIG. 2( b ) (square) and a plot of the height variation during the time (principal plot);
  • FIG. 3 shows the functionality of the “dispenser gun”: discharge at angled direction, distribution of liquid and lateral simultaneous shifting, liquid linear patterning in different positions, and specifically in:
  • FIG. 4 shows more implemented functionalities: multiple distribution and transport and “dispenser gun” activation for the distribution of high capacity by means of laser scanning on the LN surface, in particular:
  • FIG. 5 shows the pico-liter distribution on micro-engineered LN substrate, and in particular:
  • FIGS. 1( a ) and 1 ( b ) The apparatus according to the invention is shown in FIGS. 1( a ) and 1 ( b ).
  • a liquid drop 150 or a liquid film is deposed on a slide 110 , while an upper plate 120 is at a distance D from the slide by electrically isolated spacers 140 .
  • the upper plate 120 is a z-cut LN wafer (Lithium Niobate) (see section of methods for details concerning the preparation), for example of 500 ⁇ m of thickness.
  • the spacers can be more or less thermally conductors, allowing a greater or lesser activation of the drops (see later on).
  • laser CO2 infrared source
  • the heated tip source 130 ′ is in contact with a LN crystal 120 ( FIG. 1( b )).
  • the laser and the tip can be moved so as to induce local punctiform point-like thermal stimuli.
  • the distance between the slide 110 and the plate 120 is, for example, of 1 mm.
  • the z-cut LN crystal reacts to the thermal stimuli by forming an electric potential through its two surfaces (z+, z ⁇ ) due to the piezoelectric effect.
  • the pyroelectric effect consists in the change of spontaneous polarisation ⁇ Ps consequent to a temperature variation ⁇ T [29].
  • the crystal Ps is completely screened by the charge of external shield and no electric field exists.
  • the electric field has an attractive force on a liquid as shown in FIG. 1( c ).
  • the electric potential is due to the electric effect induced on the streamlined substrate by the thermal stimuli operated by the heated tip.
  • thin jets of liquid can be released by a conical tip structure (similar to the Taylor cone usually utilized in the electro-spray; nevertheless, in the present case, the liquid is not conductive, consequently there is not exactly the Taylor cone regime) [15-16-17].
  • This angle is univocally defined both by the liquid cone generated by a drop and by the liquid cone generated by a liquid film, the starting angle being always measured with respect to the substrate or the surface of the remaining liquid parallel to the substrate (see i.e. FIGS. 1 ( e ) and 2 ( b )).
  • FIG. 1( d ) A typical liquid bridge is shown in FIG. 1( d ).
  • the different contact angles at the upper and lower solid-liquid interfaces are to be noted, what is indicative that the liquid bridge is formed between the two materials with different wettability properties.
  • the second case (II) is more important: if the separation D is over the critical value, a stable liquid bridge cannot be stabilised between the plates.
  • the present invention has been reached by searching a way for using this instability with the aim of dosing and distributing the liquid drops.
  • FIGS. 1( e ) and 1 ( f ) the typical situations of liquid discharge for two different liquids are shown, almond oil and PDMS (poly-dimethyl-siloxane) respectively. Due to the high viscosity, the emission liquid cone is continuous.
  • FIGS. 2( a ) and 2 ( b ) demonstrate the distribution of almond oil nano-liter drops from a liquid film and from a sessile drops reservoir, respectively (see methods section).
  • a heated tip has been utilized, whereas, for the sessile drop, the heating has been stimulated by the laser in the infrared zone.
  • the dynamic evolution shows the liquid deformation in both the situations and it is possible to observe from the sequences (not shown) how the film and the drop heights grow under the EHD force action.
  • FIGS. 2( c ) and 2 ( d ) traces of liquid volumes transferred from the substrate as a function of time (square) and the height change (principal plot) during the discharge are shown.
  • the rate is approximately equal to 30 nL/ms.
  • the total volume transferred to the pending drop is 160 nL.
  • the drop acts as a dispenser gun with a rate of repetition that depends on the liquid response to the EHD force. It can be observed that, after the formation of the Taylor cone, in order to permit the first discharge, the dispenser gun shoots periodically liquid drops if the electric field is still active. The period of discharge has been of 50 ms. The cycle is repeated few times during the cooling.
  • FIG. 2( b ) which has been obtained utilising a CO 2 laser (but a similar result can be obtained other laser or other electromagnetic radiation sources) it is possible to proceed to the complete extraction of the liquid from the drop reservoir. This fact could be due to the improved mechanism of heating efficiency.
  • the initial volume was of 180 nL while the total final volume transferred to the photogram in FIG. 2( b ) was 164 nL and the remaining drop was 16 nL.
  • the discharge period has been of 200 ms while the volume transferred in each discharge has been estimated to be 3 nL.
  • the movement of the heated tip or of the laser permits, for example, to change the emission direction of a drop in a large solid angle as shown in FIG. 3( a ).
  • the region with the highest electric field follows the tip movement.
  • Angles of discharge out of axis reach in this case values until about 20°. This may give the possibility to dispense liquids in an area of 23 mm 2 even if the reservoir drop maintains a fixed position. More large angles imply movement of the reservoir drop, as described in the following.
  • the “dispenser gun” is moved at the same time as it is discharged in a continuous manner allowing the liquid patterning. In this case it is important to select conditions in which dragging the drop in different positions is possible, as described in the following.
  • the “dispenser gun” can be easily moved, by simply moving the heated tip. Nevertheless, in the first case the sessile drop starts to move only at a critical angle. Indeed, the asymmetric deformation experimented by the drop, under the non-axial electric force, generates an unbalance of the solid-liquid interfaces tensions with a net resulting force (see FIG. 3( b )) that pushes forward the drop. This unbalance causes the drop displacement similarly to the thermocapillarity where the thermal gradient causes the loss of balance of the solid-liquid tensions. In FIG. 3( b ), how the drop movement permits the pattering is shown, by the drops distribution from the reservoir drop in three different position along a single scanning line.
  • FIG. 3( c ) shows the lateral movements (x-axis) until 1.6 mm without distribution axis interruption, and 1 mm along the y axis (the shifting along the y axis is observable since the liquid cone is better brought in focus in the final frame (base) with respect to the out-of-focus third position that is observed in the first (upper) frame).
  • a more enhancing function of the present invention is the harmonic combination of the distribution function synchronised with the drops transport, at the same time as they are continuously formed, function that is shown in the sequence of FIG. 4( a ).
  • the sequence of images in FIG. 4( a ) clearly shows the formation and the synchronised transport, on the destination substrate, of three different drops in straight line on the right side. These drops can be easily collected and managed in a microfluidic system.
  • This function may be successfully improved by selecting in an appropriate manner the position of the thermal stimuli (heated tip, in this case).
  • the beauty of the physical phenomenon is that the process seems to be auto-organised as a function of two different physical effects: EHD and thermocapillarity, but activated by an only single external stimulus. The lateral shift is activated by thermocapillarity, that pushes the drops towards colder regions (in our case left and right sides) (see FIG. 4( a )).
  • the reason why in the shown experiment the x direction is preferred depends on the geometric design of the cell.
  • the upper substrate LN is in contact with the glass at the +x and ⁇ x ends (therefore the heating exchange with the glass is larger than in air).
  • the contact with the glass permits a heat exchange that is higher along this direction than in the y direction.
  • +x and ⁇ x sides are equivalent but if the heated tip source is not symmetrically positioned, in axis, with respect to the bottom of the reservoir drop, the liquid discharges have a moment with horizontal components that dynamically pushes the liquid preferably along the axis of the device (right side).
  • the angle in this case, is clearly visible from the image and it is of about 11° with respect to the normal at the substrate.
  • the laser beam has been directed at three different reservoir drops (see FIG. 4( c )) stored on a glassy substrate. The drops have been sequentially activated. An elevated distribution of volume is possible by separating the laser beam so as to obtain a parallel emission from many “dispenser guns” (thus accelerating the distribution process).
  • This regular structure permits to form some cones starting from the liquid that will spread itself exactly over and in correspondence of the hexagons.
  • a liquid PDMS layer has been spread over the glassy substrate.
  • thermal stimuli in a flexible manner through the use of a laser or large heating
  • the formation of three tank drops has been demonstrated in correspondence of the hexagons having a lateral separation of 200 micrometers.
  • PDMS is more viscous
  • liquid filament and unstable liquid bridges have been formed [30], as clearly visible in FIG. 5( a ).
  • 400 pL of pending drops have been clearly distributed in the exact position corresponding to the geometry of the PPLN sample (see FIG. 5( a )).
  • the system according to the invention can be utilized in different configuration so as to permit the drops distribution and their patterning.
  • a single or multiple “dispenser gun” can be obtained from one or more thank drops, preliminary obtained by processes of wettability modelling (spatial modulation of poling or thermal stimulus) on the lower substrate.
  • the substrate to be modelled is not the same dielectric polar functionalized crystal.
  • the substrate on which the liquid is laid down could be a dielectric plate (so as to avoid field perturbations) or film 160 inserted between the glass 110 and LN 120 , in order to intercept the liquid drops as shown in FIG. 5( b ).
  • a geometric design may be obtained as formed by the separated drops even with the substrate shift, as shown in figure. In principle, every geometrical figure can be realized.
  • the glassy plate 110 may house through micro-pores 190 and micro-tubes 180 to dose the distribution liquid in the reservoir drops. Besides, the liquid may be sucked from aspiration ducts if one wishes the immediate interruption of the distribution action.
  • the actual level of technology will allow, by means of computer and control electronics, the total implementation of this integrated configuration of the method according to the invention for distributing and modelling a liquid material.
  • the two starting and destination surfaces are both pyroelectric surfaces, so as to create a reciprocal distribution of the liquid between the two surfaces. This may be useful in mixing processes.
  • the z-cut LN crystals show uniform polarisation.
  • the spontaneous polarisation of LN crystals can be reversed by a polarisation process with electric field (EFP) [25], thus allowing the fabrication of periodically polarised LN crystals (PPLN).
  • EFP electric field
  • An external tension that goes over the coercive field of the material (about 21 kW/1 mm) has been necessary to invert the ferroelectric domains and the inversion selectivity is usually assured by an appropriate model of resist generated by photo-lithography.
  • FIG. 5( a ) the image obtained at the optical microscope of two PPLN samples produced by the same Inventors by “Electric Field Poling” (EFP) is shown.
  • the samples consist in a square matrix of bulk reversed domains with a period of about 200 micrometers along both the x and y directions.
  • the pyroelectric coefficient sign is reversed according to the inverted ferroelectric domains [29].
  • the power modulation in the range of 0-100% has been possible thanks to an external tension of 0-5 V.
  • the laser beam diameter has been of 4 mm.
  • the beam can be focused through suitable lens so as to obtain the desired beam dimension in the diffraction range of about half wave length (5 micrometer).
  • the laser has been assembled on a x-y translational stage.
  • the sphere head was about 25 cm apart from the LN sample.
  • a simple tip has been utilized for heated welding/soldering.
  • the diameter was of 1 mm.
  • the maximum operative temperature was 250° C.
  • the temperature has been measured by a temperature probe (thermocouple) in order to have a preliminary indication of the maximum temperature reached on both LN crystal faces.
  • the measurement equipment is composed by a white lamp, a neutral density filter and a lens of images formation for visualising in a high rate CMOS camera the process of Taylor cone deformation and the drops ejection.
  • the CMOS camera capturing 125 frame each second at the 1280 ⁇ 1024 resolution with pixel area of 12 ⁇ 12 micrometer, is utilized with two different lens for comprehending the fundamental dynamic of this process.
  • the method according to the present invention is applied in many industrial, scientific and technological fields; the nano-drops production is, in fact, of principal interest, for example, in all the sectors that treat ink-jet printing, distribution or deposition of organic, inorganic or biological inks, micro-fluids, electrospray, drug delivery, and combinatory chemistry.
  • the particularity of the method, according to the invention is the great flexibility that characterises the configuration lacking in electrodes in which the electric forces are generated by the heating induced by the utilized source directly on the interested substrate.

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US13/265,720 2009-04-22 2010-04-21 Device for controlled distribution of micro- or nano-volumes of a liquid based on the piezoelectric effect in functionalized materials, without using external electric sources Expired - Fee Related US9221047B2 (en)

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ITRM09A0187 2009-04-22
ITRM2009A000187A IT1393855B1 (it) 2009-04-22 2009-04-22 Dispensatore elettrodinamico di liquidi in quantita' micro/nano-litriche basato sull'effetto piroelettrico in materiali funzionalizzati, senza l'impiego di sorgenti elettriche esterne.
ITRM2009A000187 2009-04-22
PCT/IT2010/000172 WO2010122592A1 (fr) 2009-04-22 2010-04-21 Dispositif de distribution contrôlée de micro ou nanovolumes de liquide sur base de l'effet piézoélectrique dans des matériaux fonctionnalisés et sans recours à des sources électriques externes

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US20160008813A1 (en) * 2013-03-15 2016-01-14 Siemens Healthcare Diagnostic Inc. Microfluidic distributing device
US10105701B2 (en) 2013-03-15 2018-10-23 Siemens Healthcare Diagnostics Inc. Microfluidic distributing device

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